Ciprofloxacin Ophthalmic Solution
»Ciprofloxacin Ophthalmic Solution is a sterile,aqueous solution of Ciprofloxacin Hydrochloride.It contains not less than 90.0percent and not more than 110.0percent of the labeled amount of ciprofloxacin (C17H18FN3O3).
Packaging and storage— Preserve in tight containers protected from light,at room temperature.
Identification— Dilute a volume of Ophthalmic Solution with water to obtain a test solution containing about 3mg of ciprofloxacin per mL.Prepare a Standard solution of USP Ciprofloxacin Hydrochloride RSin water containing about 3.5mg per mL.Proceed as directed in Identificationtest Bunder Ciprofloxacin Hydrochloride,beginning with “Separately apply,as 1-cm bands,”except to use 3µLeach of the test solution and the Standard solution instead of 5µL.The specified result is obtained.
Sterility á71ñ— It meets the requirements when tested as directed for Membrane Filtrationunder Test for Sterility of the Product to be Examined.
pHá791ñ: between 3.5and 5.5.
Assay—
Mobile phase— Prepare 0.005Mtetrabutylammonium phosphate,and adjust with phosphoric acid to a pHof 2.0.Prepare a degassed and filtered mixture of this solution and methanol (750:250).Make adjustments if necessary (see System Suitabilityunder Chromatography á621ñ).
Standard preparation— Dissolve an accurately weighed quantity of USP Ciprofloxacin Hydrochloride RSin water to obtain a solution having a known concentration of about 0.14mg per mL.
Resolution solution— Dissolve a quantity of USP Ciprofloxacin Ethylenediamine Analog RSin a portion of the Standard preparationto obtain a solution containing about 0.01mg per mL.
Assay preparation— Transfer an accurately measured volume of Ophthalmic Solution,equivalent to about 6mg of ciprofloxacin,to a 50-mLvolumetric flask,dilute with water to volume,and mix.
Chromatographic system (see Chromatography á621ñ)—The liquid chromatograph is equipped with a 280-nm detector and a 4.6-mm ×25-cm column containing packing L1.The flow rate is about 1.5mLper minute.Chromatograph the Resolution solution,and record the responses as directed under Procedure:the relative retention times are about 0.8for the ciprofloxacin ethylenediamine analog and 1.0for ciprofloxacin,and the resolution,R,between the ciprofloxacin ethylenediamine analog peak and the ciprofloxacin peak is not less than 1.5.Chromatograph the Standard preparation,and record the responses as directed under Procedure:the capacity factor,k¢,for the ciprofloxacin peak is between 1.5and 6,the column efficiency is not less than 500theoretical plates,the tailing factor for the analyte peak is not less than 0.9and not more than 2.0,and the relative standard deviation for replicate injections is not more than 2%.
Procedure— Separately inject equal volumes (about 20µL)of the Standard preparationand the Assay preparationinto the chromatograph,record the chromatograms,and measure the areas for the ciprofloxacin peaks.Calculate the quantity,in mg,of ciprofloxacin (C17H18FN3O3)in each mLof the Ophthalmic Solution taken by the formula:
(331.34/367.81)(50C/V)(rU/rS),
in which 331.34and 367.81are the molecular weights of ciprofloxacin and anhydrous ciprofloxacin hydrochloride,respectively;Cis the concentration,in mg per mL,of USP Ciprofloxacin Hydrochloride RSin the Standard preparation,calculated on the anhydrous basis;Vis the volume,in mL,of Ophthalmic Solution taken;and rUand rSare the peak responses obtained from the Assay preparationand the Standard preparation,respectively.
Auxiliary Information— Staff Liaison:Behnam Davani,Ph.D.,MBA,Senior Scientist
Expert Committee:(PA7)Pharmaceutical Analysis 7
USP28–NF23Page 479
Phone Number:1-301-816-8394